反応 #80429

ord-859bedd244794340b240a80076a55878

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with ethyl acetate
  2. 2
    乾燥The extract was dried over anhydrous magnesium sulfate
  3. 3
    workup.DISTILLATIONthe solvent was distilled away under reduced pressure
  4. 4
    抽出extracted with chloroform-methanol

実験手順

2-((3-Methyl-4-(3-aminopropylthio)-2-pyridyl)methylthio)1H-benzimidazole (2.0 g) was dissolved in dimethylformamide (20 ml) and thereto were added ethylene bromohydrin (0.83 g) and potassium carbonate (1.25 g). The mixture was stirred at 60°-70° C. for 2 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and the solvent was distilled away under reduced pressure. The residue was subjected to column chromatography and extracted with chloroform-methanol to give 2-((3-methyl-4-(3-(2-hydroxyethylamino)propylthio)-2-pyridyl)methylthio)-1H-benzimidazole.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05616581uspto-grants-1997_04